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Method for separating diphenic acid from tower bottom waste for preparing benzoic acid

A technology of bibenzoic acid and benzoic acid is applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., to achieve the effects of high economic value, little environmental pollution, and easy separation and purification

Inactive Publication Date: 2013-09-04
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In my country, Shijiazhuang Oil Refining and Chemical Co., Ltd. and Tianjin University have jointly developed a method for recovering compounds such as benzoic acid, benzyl benzoate and fluorenone in the still raffinate by using a combination of flash distillation and vacuum distillation, and established a production line, but there is no further recycling of the bottom waste after vacuum distillation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Raw materials and reagents: waste at the bottom of the tower, the waste at the bottom of the tower after rectification of benzoic acid by Shijiazhuang Oil Refining and Chemical Co., Ltd.; sodium carbonate, chemically pure; ethanol, chemically pure; toluene, chemically pure; hydrochloric acid; chemically pure.

[0026] Steps:

[0027] Add 100g of tower bottom waste and 500mL of ethanol into a 1000mL three-neck glass flask, heat, and stir at 65-70°C for about 1.5h; stop heating, cool to room temperature, then add 50mL of water into it, stir to make it evenly mixed, and pump Filter to obtain black viscous solid (1) and brown-black filtrate (1). Add 700 mL of water to the brown-black filtrate (1), stir and mix evenly, let stand for 1.0 h, and filter with suction to obtain khaki solid (2) and light yellow waste liquid (2). Add 1500 mL of water and 35 g of sodium carbonate to the khaki solid (2), stir at room temperature for 1.0 h, and filter with suction to obtain khaki sol...

Embodiment 2

[0033] Raw materials and reagents: with embodiment 1.

[0034] Steps:

[0035] Add 100kg of waste at the bottom of the tower and 500L of ethanol into a 1000L reactor, heat, and stir at 65-70°C for about 1.5h; stop heating, cool to room temperature, then add 50L of water into it, stir to make it evenly mixed, and then filter with suction , to obtain black viscous solid (1) and brown-black filtrate (1). Add 700L of water to the brown-black filtrate (1), stir and mix evenly, let stand for 1 hour, and filter with suction to obtain khaki solid (2) and light yellow waste liquid (2). Add 1500 L of water and 35 kg of sodium carbonate to the khaki solid (2), stir at room temperature for 1.0 h, and filter with suction to obtain khaki solid (3) and brown transparent filtrate (3). Add dropwise hydrochloric acid to the brownish-yellow transparent filtrate (3) to adjust the pH value to 1 to 2, let stand, and suction filter the filtrate after it is cooled to room temperature to obtain 28.0...

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Abstract

The invention provides a method for separating diphenic acid from tower bottom waste for preparing benzoic acid, and in particular relates to a method for extracting mixed diphenic acid from tower bottom waste for preparing benzoic acid by direct liquid phase oxidation of toluene and separating and purifying 3-phenyl benzoic acid and 4-phenyl benzoic acid. Any high-toxicity organic solvent and any catalyst are not used in the reaction process; the purification process is simple in operation; and the toluene serving as an organic solvent in the reaction process and the purification process can be recycled in a rectifying mode, and ethanol serving as an organic solvent can be recycled by rectification after simple treatment. The method further expands the utilization range of the tower bottom waste for preparing the benzoic acid by direct liquid phase oxidation of the toluene, and has the advantages of simplicity and convenience in operation, easiness in separation and purification of the product, low environmental pollution, low cost, high economic value and the like.

Description

technical field [0001] The present invention relates to aromatic organic compounds, in particular to a method for extracting mixed biphenylformic acid from the bottom waste of benzoic acid prepared by direct liquid phase oxidation of toluene and separating and purifying 3-phenylbenzoic acid and 4-phenylbenzoic acid method. Background technique [0002] Benzoic acid is an important organic chemical raw material, which is widely used in industrial production such as food additives, pharmaceutical intermediates, cosmetics and polymer materials, especially as a raw material for the production of caprolactam and phenol. The annual consumption in the world is just 100 More than 10,000 tons. At present, the annual output of benzoic acid in the world is more than 2 million tons. Benzoic acid is initially obtained by dry distillation of benzoin gum or hydrolysis of alkaline water, and it can also be obtained by hydrolysis of hippuric acid or decarboxylation by hydrolysis of phthali...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C63/331C07C51/43
Inventor 张昭乔鹏伟张鑫吉轩韩卫东
Owner SHANXI UNIV
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